Double-nitrid composition of matter.



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SAMUEL rnacocmmr cmcaeo, nniuois, assiciionlro .rnrsanarzonar. asmcnn: 'I'UZRAL conronlrrron, or new some, N. Y., A coaronarron on NEW YORK.

bonersmanic comrosirtou on Mariana.

1V0 Drawing.

description of the invention, such as will en able others skilled in the art to which it appertains to make and use the same.

This invention relates to compositions at matter consisting of double nitride of metals, or of metal andv a lnon-inctal, or of an alkali earth inetaland anon-metal, and'has for its object to produce such compositions ina' cei'tain and inexpensive manner.' i I To theseends the invention consists in the novel compounds or compositions of matter rnore fully hereinafter disclosed and particularlyjointed o t in the claims.

In order that mvsaid compounds may be more clearly understood. it is said :ln the process of making silicon carbo-nitrid (Sm- N I observed that the temperature of the formation of the double nitrid is so nearly that of its dissociation, that the proc' ess of producing said double nitridbecamc one of exceptional refinement in carrying it,

' means of double nitrids of a metal and a non-metal in which silicids or silicon carpounds such as (1) (lil hl'l Si lsl milaim, (3) (I(,N),.Si,N,,

as Well as other like compounds in which other metals, alkali earth metals and nonmetals may be substituted for those mean tioned, other, Words, 1 discoye ed that it Was'pos'sible to'sub stitute silicon for car bon in the-older processes it metal oxide Specification of Letters Patent. A ucati ii'fiiea ma 31, 1913. Serial No. 770,932.

Patented Jan. 5, 1915.

were mixed with the charge of carbon and silica.

In carrying out my process, I provide a mixture of carbon, silica and an oxid of a metal, using either a natural compound such as feldspar, ora mixture of oxids in such proportions that there will be present in the charge sufiicient carbon to effect the reduction of substantially all the silica present, and, to cause the formation of the higher carbid of silicon Sic... This latter carbid is not very stable at the temperature of its formatiombut it readily reacts with alumina,,calcium oxid, etc... to form silicids in accordance with the followingz These reactions, (or similar reactions in which other metals are substituted for the aluminum. calcium or potassium) are by my process effected in an atmosphere ofnitrogen. Further, the metal silicids produced being unstable, ordinarily tend to break down, substantially as folloxvs,

(1) Ailing:A l Si l-llil (2) 'Ca fi li :(hi..Si ,l-Ca (3) K Sn K Si -i-K, This dissociation of these silicids is more or less aided by the presence of uncombincd :carbom-Which forms carbids with the metal liberated. In the presence of nitrogen,

, however, I have found that these SlllClllS (lecompose into double nitrids of a metal and a non-metal, substantially as follows bids are utilized, and thus produce comvery useful one to' employ in "the beginning.

:Accerfli'ngly, in the operation of my process I take the required mixture of carbon,

7 producer gas metal oxids, and silica, as separate substances, or as any natural or artificial compound or mixture of the same, and heat such mixture by any suitable means in an atmosphere of nitrogen. Preferably, I cake or briquet the mixture, and make use of a containing a low percentage of carbon dioxid as a source of nitrogen; the said producer gas being passed over or through the cakes or mixture as the same is heated. The temperature required is from 1600 to 2000 G. depending upon the velocity with which the producer gas is passed through or overthefurnace mixture. first step in the reaction produces carbon monoxid CO as a gaseous reaction product, and the reaction velocity is governed by the partial pressure of this said carbon monoxid exist in the furnace atmosin order to hasten this velocity same time increase the above phere ;hence, and at the range of temperature differences, I keep the partial pressure of this gaseous reaction product as low as possible as by sweeping the producer gas somewhat rapidly through or over the the furnace under treatment. I

I preferably use any suitable furnace employing electricity having opposed electrodes as a source of heat, and provided with suitable well known devices for a continuous feeding of the charge and for the removal of the furnace product.

In carrying out the above process I have found evidences of a nitrogen compound corresponding to the formula AI N Si N but could not prove it to be anything more than a mixture of the two compounds AI N and Si,,N,, which may have resulted from excessive temperatures in particular portions of the furnace. However, although such compounds are included in my discovery, yet it is important to avoid the formation of such compounds or mixtures, because they require a greater expenditure of energy, and fix a much less quantity of nitrogen than do the higher nitrids. Such avoidance can be accomplished by watching the operation,

charge in and seeing that the temperatures are as even as possible all over the reaction zone.

In making up the a desirable mixture a consist in feldspar and phosphate rock in such proportions that the silica of the feldspar is supplied with ample calcium oxid from the phosphate rock to form the above calcium silicid, for in such case not only is the silica, alumina and calcium oxid of the minerals thus utilized to fix nitrogen, but the potassium of the feldspar, and the phosphorus of the phosphate rock are first both volatilized in the form of oxids, and then converted into carbo-nitrids furnace charge I find particular class of higher carbids, for it is these same higher carbids that are found to effect the dissociation in the cyanamid process of fixing nitrogen. Such higher carbids are 5H),, ZnC, A1 0 CaC. They invariably give rise in the reaction to a carbon valency corresponding to (LIL, and this said valency will cause for example tl1 compound Al,N,.Si .,N, to be produced 1f the temperature not too high instead of the compound AhN Si N )f course, if such higher carbids as ZnC, Al C CaC, etc., are substituted for the silicon carbid SiC in the above reactions, then the double nitrids produced will be correspondingly changed. In other words, in the presence of nitrogen I may employ LWO oxids of metals. instead of an oxid of a metal, an( an oxid of a nonmetal, and produce the above higher cal-bids of the metals during the reaction, which will immediately break down, and give rise to double nitrids of thecorresponding metals present, instead of double nitrids of a metal and a non metal.

t is obvious that those skilled in the art may vary the steps without departing from the spirit of my invention, and therefore I do not wish to be limited to the above disclosure except as may be required by the claims.

lVhat I claim is l. The herein described new composition of matter containing a double nitrid of a metal and anon-metal, substantially as described.

2. The herein described new composition of matter containing a double nitrid of an alkali earth metal and anon metal, substantially as described.

3. The herein described new composition of matter consisting of a double nitrid of calcium and silicon, substantially as described.

In testimony whereof I aflix my signature,

presence of two witnesses.

SAMUEL PEACOCK. 

